Massive boron carbid and process of making same.



No. 869,114. PATENTED OCT. 22. 1901.

' s. A. TUCKER. MASSIVE BORON GARBID AND PROCESS OF MAKING SAME.

nrmouxou FILED no. 19, 1906. V

' 2 SHEETS-SHEET 1-..

' [NVENTOR 9M 0%? s. A. TUCKER.

MASSIVE BORON GARBID APPLIOATI AND on NI.

PROCESS OF MAKING SAME.

PATENTED OCT. 22- 1907.

SAMUEL A. TUCKER, on NEW YORK, Y., AssieNoR TO ELMER A. SPERRY, or

NEW YORK, N. Y.

MASSIVE BORON CARBID AND PROCESS OF MAKING SAME.

Specification of Letters Patent.

Patented Oct. 22, 1907.

Application filed December 19, 1906- Eerial No. 3%.607-

To all rrlzom ii. may concern:

Be it known that l, SAMUEL A. TUCKER, a citizen of the United States, residing at New York, in the county of New York and State of New York, have invented new and useful Improvements in Massive Boron Carbid and Processes of Making Same, of which the following is aspecilicatiou.

The object of my invention is the cominerciabproduction of pure or practically pure boron carbid-l-3,,C, lllfliilllt1(tl1l'l'llg it from commercial and comparatively inexpensive compounds of boron and producing it directly in the electric furnacc,-that is, avoiding the expensive process of separating it from metals or other bodies in which it is suspended or with which it is intimately associatul, as has been the practice heretofore with the minute quantities that have been produced. Furthermore, to produce this product in a more available form as to physical character, meaning; by this as a ponderable mass or masses instead of a fine dust or impalpablc powder found upon microscopic examination to consist of minute crystals. h'y new massive boron carbid has a specific gravity of about 2.7.

lrcvious methods employing a boron compound have found it necessary to associate the compound with other bodies in which the product is dissolved,see Moissans solutionof boron and carbon in certain metals at electric furnace temperatures, this having been recommended by him as the most suitable method for its preparation, Or again, where the carbid becomes intimately associated with the foreign bodies,-soe Bloissans silicate of alumina and boric acid reaction where the product is intimately associated with silicon carbid. Where the carbid is dissolved in metals, laborious and expensive solutions of the metals are necessary to reclaim thelittle powdered carbid, which even then is so intimately mixed with graphite as to blacken the fingers. .loly and h'liihlhauser produce a mixture of bodies, the latter failing to identify the carbid assuch, denominating the product as a borid of carbon--30.

The dust-like powder resulting from reactions with amorphus boron and carbon form no part of tliepresent invention.

The pure boron carbid produced by the present process has many uses in the arts. It is available as a highly refractory material, it being an electrical conductor; from it, incandescent filaments and high temdum, easily scratching or reducing'either, having been used to produce facets upon diamonds. This hardness would be of very little value, were it not for the entirely new form. in which the substance is produced by my process, namely, in the massive state, for in this form it has no definite unit quantity or shape, as for (it) instance, the plate crystals of carborundum, nor is it brittle or fragile, as is this crystal; at the same time, it is definitely harder. Pieces of this substance are, therefore, available for a large number of uses; for instance, they have been set in place of boi'tri, carbon (t5 and diamonds in the diamond drill; they have been used for stone dressing and as glass cutters; also for dressing emery and carborundum wheels. Pieces of this substance have been drilled for use as dies in place of carboiis and diamonds for wire drawing. also be used as an alloy for cominingling with metals for producing changed or altered characteristics in such metals. twill also be readily understood that the physical structure and the fact that I may produce. the

B C may product in the massive form has a very pronounced bearing on many other of its uses, for instance, its use as an electrical conductor and as an electrode for electrolytic work, as stated.

As illustrating one method of its preparation, reference is hereby made to the accompanying (lI'LUilHfJS Si) Fig. 2 shows a vertical S5 The material consisting for instance of carbon and anhydrous boron oxid (B 0 preferably well comminried in predetermined proportions as to the boron and carbon constituents, is placed within any form of suitable inclosui'e, as for instance the chamber 5 made of refractory substance, such for instance as pure graphite and preferably capable of sustaining a pressure without undue leak-ago, being closed by cap (5, which may be supplied with an upwardly extending, stem or tube 7. This cell or inclosuie is placed within a cavity in an electric furnace 8, and packed with electric conducting, but resisting material, such as carbon or boron carbid partic is 9. The terminals 10, 10, lead to the secondary of the transformer ll supplied from an alternating current source 12, iii the current of which is a regulator, or reactance coil, 13, tliecore of which is operated by the'levei' 14, actuated by any suitable filltoinatic device, as for instance, the clock-w01k'15, or may be operated by handle 16.

Means are provided whereby the contents of the chamber 5 may be brought under suitable pressure "during the reaction or other period, and to this end the upper end of the tube 7 is provided with a suitable 5 closure or valve illustrated by the ball 17 held in place by lever and weight 18 which are capable of being thrown back out of position, as is shown in Fig. 3, whereby a rod 19 or other suitable stirrer, maybe introduccd and operated. I It is found for some purposes'preierable to mix the .1

ingredients in such proportions that the boron compound is present somewhat in excess. I The process in volving the use of excess of the boron element is found advantageous in yielding a purer product, and one .15 freer from admixed graphite and other impurities, and

also aiding to yield massive bo'ron carbid, which is a form herein pointed out for the first time. 1 r 7 It will be readily understood that other means can be employed, such for instance as a pump for placing 2O the contents of chamber Sunder pressure and for controlling the: pressures within such chamber.

Having thus described one form of the apparatus, the method of operation will be obvious from the foregoing. The mixture having'been placed in' the chamher 5', the heat is brought to a point where the boron oxid melts into a glassy and somewhat viscous mass 20. At this point in the operation it may be desirable that the materials be stirred which may be accomplished in any; suitable manner, for instance the furnace as a whole-may be moved or the inclosure 5 itself may be moved in the loose rcsi'sting material 9, or. the contents may be directly stirred, as shown in Fig. 3, during which time the temperature may be raised to the point where the reaction takes place. It

may be stated of this reaction that it is perfectly definite and with proper temperature very, vigoroua'the gases coming from the chamber in considerable volume easily serving through the adjustable ball-valve mech anism 17 and 18 to control the pressures within the 40 chamber. I

I find that the temperature and its distribution is 1 important and for some purposes it desirable that the chamber 5 or its equivalent be somewhat elongated I and that it be subjected to-a non-uniform temperature i so that in this manner upon removal of the product it may =-be scgrega ed into masses produced at critical temperatures, have discovered that in this I way carbid possessing peculiar physical characteristics may be obtained and separated from that which posscsses other characteristics or forms. In this manner I have produced pondcrable masses of practically pure I cooling 1 have made the discoverythat crystals, re-

gardless of their exact method of production are larger with a definite tendency to freedom from fracture and have provided as one means of producing slow cooling, the current regulating mechanism 13, 14, 15, and 16, which may be actuated automatically to perform this function. I I

The ponderable masses having a metal-like fracture which are herein described for the first time and conboron carbid. I

My process is not limited to the steps or features in the order named, nor to the apparatus or materials described herein, nor in any particular other than is set forth in the accompanying claims taken in connection with the specification.

I claim:

1. The process which consists in bringing a boron compound and carbon to the reacting temperature under conditions which produce practically pure boroncarbid.

2. The process which consists in bringing a boron oxid and carbon to the reacting temperature under conditions which produce practically pure boron carbid.

a boron compound in excess to the reacting temperature "undcr conditions which produce practically pure boron car-bid. I

4. The process which consists in bringing a boron compound and carbon to the reacting temperature under conditions, which produce practically pure boron car-bid and then cooling the product slowly:

r 5. The process whichconsists, in bringing'a boron com pound and carbon to a non-uniform but reacting temperature under conditions which eliminate foreign bodies from of the different temperatures. I

6. The process which consists in bringing a boron compound and carbon to the reacting temperature under conditions of temperature. control and which also produce practically pure boron cal-bid.

7. The process which consists in bringing a boron compound and carbon to thereactin'g temperature under conditions which producepractically pure boronv car-bid, cooling the outer layers andallowing contraction to open up caverns within the mass, aiding thereby in producing carbid of different physical characteristics. and afterwards separating same. I

8.-'lhe method of producing practically pure boron carbid which consists in bringing a boron compound and carbon in an inclosure to -'the requisite'temperatin'e to produce the reaction and controlling the pressure within the inclosurc. I l I I 9. As a new article of manufacture a mass having a metal like fracture and a specific gravity of approximately 217 consisting of practically pure boron carbid.

10. As a new article of manufacture boron carbid having a composition substantially B C.

C. ALEX. NELSON, Fnnnnmc W. ERB.

more valuable when the cooling takes-place slowly. I I

the carbid produced and separating the reaction products In testimony whereof Lhave hereunto set my hand in,

SAMUEL is. TUCKER.

sist of practically pure B 0 may be known as massive 3. The processQwhieh consists in bringing carbon and 

